Process for the preparation of laundering compositions

ABSTRACT

A process for the preparation of a spray-dried, built, detergent-softener composition containing an ethoxylated nonionic detergent in combination with a di-higher alkyl quaternary ammonium textile softener is described which comprises the steps of (1) admixing the softener, nonionic detergent, and water to form an aqueous mixture containing a homogeneous dispersion of the softener; (2) incorporating an inorganic sodium or potassium phosphate builder in the aqueous mixture of step 1 to form a mixture containing more than 50 percent solids by weight, the temperature of the mixture being at least about 180* F. at the time the phosphate is introduced therein, and (3) spray drying the mixture of step 2.

United States Patent New York, N.Y. Continuation-impart of applicationSer. No. 587,364, Sept. 26, 1966, now abandoned.

PROCESS FOR THE PREPARATION OF LAUNDERING COMPOSITIONS 10 Claims, NoDrawings U.S. Cl 252/137, 252/152 Int. Cl Clld 1/62, Cl ld l/86,C1 1d3/06 Field of Search 252/137, 152, 99

References Cited UNITED STATES PATENTS 3,325,4l4 6/1967 lnamorato252/l52X 3,360,470 12/1967 Wixon 252/l52X ABSTRACT: A process for thepreparation of a spray-dried, built, detergent-softener compositioncontaining an ethoxylated nonionic detergent in combination with adi-higher alkyl quaternary ammonium textile softener is described whichcomprises the steps of( l admixing the softener, nonionic dctergent, andwater to form an aqueous mixture containing a homogeneous dispersion ofthe softener; (2) incorporating an inorganic sodium or potassiumphosphate builder in the aqueous mixture of step i to form a mixturecontaining more than 50 percent solids by weight, the temperature of themixture being at least about 180 F. at the time the phosphate isintroduced therein, and (3) spray drying the mixture of step 2.

PROCESS FOR THE PREPARATION OF LAUNDERING COMPOSITIONS This is acontinuation of Ser. No. 587,364, filed Sept. 26, 1966, now abandoned.

A PROCESS FOR THE PREPARATION OF LAUNDERING COMPOSITIONS This inventionrelates to the preparation of laundering compositions and moreparticularly to a process for preparing spray-dried granular launderingcompositions.

The application of Harold Eugene Wixon filed Aug. 2, I966 bearing Ser.No. 576,493 entitled LAUNDERING COMPOSI- TIONS, now US. Pat. No.3,360,470, which is incorporated by reference herein, concerns itselfwith a novel composition comprising a quaternary ammonium textilesoftener and an alkali metal carboxymethylcellulose. The function of thesoftening agent is to render fabrics and textiles soft" with respect tohandle, hand, touch, or feel. However, due to the presence of coloredcolloidal particles in most water supplies, these cationic softeningagents, while softening, have a tendency to yellow fabrics and,therefore an antiyellowing agent, i.e., the alkali metalcarboxymethylcellulose, is introduced in sufficient amount to inhibitthe yellowing effect. This particular softener composition can be usedtogether with a detergent composition in the wash cycle rather thanhaving it introduced in the rinse cycle, which is generally the casewith fabric softeners.

The practice has been to form the components of the softener compositioninto granules and mix these granules with detergent composition granulesto produce a commercial package. This is usually accomplished by using athree-step process, which merely means that the softener granules andthe detergent granules are prepared separately by crutching and spraydrying and the two kinds of granules are subsequently blended to producethe product. The three-step" process as the term is used in theindustrial sense is not given a literal interpretation. Actually, thefirst two steps are complete processes within themselves for crutchingand spray-drying a particular composition, in this case a softener ordetergent composition. The third step is concerned with the blending ofthe two components.

Although the three-step process produced a satisfactory product, it wasuneconomical in that either two sets of crutching and spray-dryingequipment were needed if preparation of the softener and detergentgranules was to take place simultaneously or, in the alternative, thepreparation time had to be extended if the same equipment was to be usedfirst for one type of granule and then for the other type of granule. Inboth cases, of course, a blending machine was still necessary to mix thegranules. It can be readily seen that the elimination of one of thecrutching-spray drying procedures and the blending step not only wouldsave equipment but would save time solids eliminate some material waste.

A one-step process was then attempted in order to eliminate the need forextra equipment and cut the process time by preparing the softener anddetergent in a form whereby each granule contained by proportionateshare of softener and detergent. It was felt that this process wouldalso reduce segregation and contribute to a higher uniformity ofproduct.

In order to carry out the one-step process, softener and detergentcomponents as disclosed in U.S. Pat. No. 3,360,470 referred to above,were mixed in a crutcher under the assumption that after crutching, themixture of components could then be spray-dried in a conventionalmanner; however, it was found that when more than 47 percent solids (byweight based on the total weight of the ingredients introduced into thecrutcher) were present in the crutcher substantially irreversi blegelation occurred to the extent that spray drying could not be effected.The one-step" process was, therefore, unfeasible in an industry wheregenerally more than 47 percent solids and preferably about 59 or 60-65percent solids must be spray-dried in order to produce an economicalproduct. In

view of the problem of gelation, it became apparent that it was moreeconomical to prepare a softener-detergent product from the foregoingthree-step" process than to use a onestep" process with 47 percent orless solids, especially in view of the fact that the gelation was foundto be substantially irreversible even though water dilution and heatingwere applied to break the gel.

It is, therefore, an object of this invention to provide an economicalone-step process for the preparation of spraydried softener-detergentgranules based on an amount of crutcher solids which is more than 47percent by weight and preferably about 59 to about 65 percent by weight.

A further object is to provide a process whereby the spraydriedsoftener-detergent granules are such that the softener and detergentcompositions are combined in each granule in a homogeneous relationship.

Other objects and advantages will become apparent from the followingdescription of the invention.

In accordance with the invention, a one-step process has been found forpreparing a spray-dried granular softener-detergent composition whereineach granule is composed of a homogeneous mixture of softener-detergentcomponents comprising:

a. admixing water, a water-soluble nonionic detergent, and a quaternaryammonium salt at a temperature of at least 180 F., wherein thequaternary salt is homogeneously dispersed therein and the mixturecontains more than 47 percent solids by weight;

b. introducing an alkali metal phosphate builder into the mixture; and

c. spray-drying the mixture.

It is preferred that at or about the time of introduction of the alkalimetal phosphate, during step (b) an inorganic water soluble diluent toprovide bulk and an alkali carboxymethyl' cellulose as an antiyellowingagent, be added. So long as the temperature of the mixture is at least180 F., and the quaternary salt is dispersed, the order of addition ofthe alkali metal phosphate and the inorganic water soluble diluent (electrolytes) is immaterial. The alkali metal carboxymethylcellulose can beadded at any point of the process.

The spray-dried product of this invention has been found exceptionallysatisfactory in the following parameters: solubility, free flow, lowdust content, storage, narrow distribution of particle sizes, bulkdensity, residual moisture content, and color. The granules, which, aspreviously mentioned, contain a homogeneous mixture ofsoftener-detergent composition, are hollow and have sufficient strengthto resist the stress and strain of handling which take place throughoutthe processing, packaging, and delivery stages of their commercial life.The final cup weight of the commercial product is preferably from about60 to 125 grams, flowability about 70 percent to about percent, andparticle size about 16 to about 60 mesh. Cup weight is based on a cupwhich holds 237 grams of water.

A more detailed description of the process of this invention follows:

The first part of the process is carried out in conventional crutchingapparatus wherein initially water, a water-soluble nonionic detergent,and a quaternary ammonium salt are introduced simultaneously or in anyorder which is desirable to the operator. The preferred order is thatstated.

All of the conventional water-soluble nonionic detergents can be used inthe process of this invention, but are preferably in liquid or pasteform. Generally, such nonionics have a hydrophobic group containing atleast 8 to 30 carbon atoms. One particular class of such detergents isthat formed by the oxyalkylation of fatty acids, alcohols, phenols,mercaptans, thiophenols, amines, and with ethylene oxide, propyleneoxide, and other related alkylene oxides. Such materials usually have atleast 5 mols of alkylene oxide, and preferably 5 to 30 mols of alkyleneoxide, depending upon the particular hydrophobic group desired.Representative of these materials are those formed by condensation ofethylene oxide with alkyl phenols or alcohols. Particularly preferredherein are condensates formed by the reaction of one mol of nonyl phenolor a mixture of C -C saturated, straight-chain, aliphatic alcohols with8 to l2mo1s of ethylene oxide, the condensates containing an average ofabout 8 to ethylene oxide groups per molecule. Some specific examples ofthis type of nonionic detergent are as follows: nonyl phenol-ethyleneoxide condensates having an average of 9.5 ethylene oxide groups permolecule; a mixture of saturated aliphatic alcohols having from 14carbons to l8 carbons in their chains and an average of 8.5 mols ofethylene oxide per molecule; tallow alcoholethylene oxide condensatehaving an average of 9 mols of ethylene oxide per molecule; and a 1:1mixture of a C and a C saturated aliphatic alcohol having an average of8.5 mols of ethylene oxide per molecule. Other alkylphenol condensatesare those of diamylphenol, p-tert-octylphenol, 2,4- dicyclohexylphenol,m-pentadecylphenol, and benzyl-ohydroxybiphenyl. Other condensates withalkylene oxide are those of tall oil, branched chain C to C,-, aliphaticalcohols, lanolin, beeswax, bis-phenols, oxidized paraffin wax,napthenic acids, and fatty acyl alkanolamides. Mixtures of various watersoluble nonionic detergents are contemplated.

The quaternary ammonium slat softener can be exemplified by thefollowing general formula:

wherein R and R are alkyl groups each containing from 1 to 3 carbonatoms; R and R are aliphatic groups each containing from 12 to 22 carbonatoms; and X is selected from the group consisting of chlorine, bromine,and methyl sulfate. These compounds are readily dispersible in water.Specific examples are as follows: distearyl dimethyl quaternary ammoniumchloride; distearyl dimethyl quaternary ammonium bromide; distearyldimethyl quaternary ammonium methylsulfate; dicoco dimethyl quaternaryammonium chloride; dimethyl arachidyl behenyl quaternary ammoniumchloride; dialkyl dimethyl quaternary ammonium chloride, the alkylgroups of which comprise a mixture consisting essentially of 24 partshexadecyl 75 parts octadecyl and 1 part octadecenyl groups; the latterquaternary ammonium chloride is also known as dimethyl dihydrogenatedditallow ammonium chloride and is particularly preferred. Mixture of twoor more cationic softener agents can be employed if desired. (The termcoco" refers to fatty acid groups formed in coconut oil fatty acids.Such acids contain from about 8 to about 18 carbon atoms per molecule,predominating in C C acids). Other examples are dimethyl ditallowhydrazinium chloride and dimethyl ditallow quaternary ammonium methylsulfate.

The proportions of the foregoing components which can be used are asfollows: waterabout 33 percent to about 43 percent and preferably about35 percent to about 41 percent; nonionic detergentabout 3.5 percent toabout percent and preferably about 4.5 percent to about 8.5 percent;quaternary ammonium salt-about 1 percent to about 6 percent andpreferably about 2.5 to about 4 percent. These percentages are by weightand based on the total weight of the initial materials as introducedinto the crutcher. The proportions of the other components will be setforth below.

It is important that the quaternary ammonium salt be homogeneouslydispersed in the mixture before the phosphate builder is added. This isaccomplished by heating or agitation caused by merely admixing thewater, nonionic, and quaternary salt or by external means. Bothagitation and heating are discussed below. The homogeneous dispersion ofthe quaternary ammonium salt bears a similarity to a melt or solution ofthe salt in the water and nonionic.

Agitation, which is preferred and practical, can be initiated before,during, or after the water, nonionic detergent, and quaternary ammoniumsalt are introduced into the crutcher.

The speed of agitation can range from about 100 revolutions per minute(r.p.m.) to about 500 r.p.m. and preferably from about r.p.m. to about400 r.p.m. and can be varied during the course of the process. The givenrates are based on the used of conventional equipment. Actually, anyreasonable movement or agitation of the mixture will suffice to carryout the process of this invention so long as it commences before or atthe same time as the addition of the second group of components,although high shear agitation is not practical.

Before introduction of the phosphate, the materials in the crutchershould be a temperature of at least about 180 F. It is preferred toinitially heat the first group of materials (water, nonionic, andquaternary salt) about 130 F. to about F; however, there is noprohibition against raising the temperature at any time before thesecond group of materials is added. The particular mode of heating isnot important and can be accomplished with whatever heating apparatus isavailable so long as the temperature can be ascertained. Once thetemperature of the mixture has been raised to at least 180 F. and thequaternary salt is homogeneously dispersed, the second group ofcomponents can be introduced into the crutcher. There is actually noupper limit for the temperature of heating the crutcher materials otherthan keeping the temperature below the boiling point of water (212 F.).However, the most practical temperatures are from about 180 F. to about200 F. and preferably from about 180 F. to about 190 F. If theternperature is less than 180 F. and particularly about F. or less,gelation occurs after one or more of the second group of components isintroduced to obtain more than 47 percent solids. It should be notedthat between 175 F. and below about F. there is a gray area in whichgelation is not sharply apparent, but is sufficient to hamper economicalspray-drying. By heating to at least about 180 F., this partial gelationis also avoided.

Once the proper temperature has been attained, and the quaternary salthomogeneously dispersed, the alkali metal phosphate, the inorganicwater-soluble diluent, and the alkali metal carboxymethylcellulose canbe introduced into the crutcher. Just as the first group of components,this second group has no particular order of introduction and eachcomponent can be introduced one at a time or the entire group can beadded simultaneously, although preferably the order stated is the orderfollowed. Agitation can be continued until a homogeneous mixture isattained.

Examples of the alkali metal phosphate builder salts are the alkalimetal tripolyphosphates and pyrophosphates of which the sodium andpotassium compounds are most commonly used. These phosphates are wellknown in the detergent art as builders and can either be used alone oras mixtures of different phosphates. More specific examples of phosphatebuilder salts are as follows; sodium tripolyphosphate; sodium phosphate,tribasic; sodium phosphate, monobasic; sodium phosphate, dibasic, sodiumpyrophosphate; sodium pyrophosphate; acid. The corresponding potassiumsalts are also examples of satisfactory builders for use herein alongwith mixtures of the salts or corresponding mixed potassium-sodiumsalts.

Of the tripolyphosphates, a low phase l material is preferred, i.e., aphase 2 tripolyphosphate associated with a maximum of about 8 percentphase 1 tripolyphosphate, the phase 1 crystalline form being a hightemperature rise material with hydrates more rapidly than the phase 2material. The preferred tripolyphosphate form is conventional for spraydry ing operation and was used in Example I, below.

In order to give bulk to the composition, an inorganic water solublediluent can be used which is exemplified by the preferred alkali metal(generally Na or K) sulfates such as sodium sulfate. These preferreddiluents generally do not provide any substantial detersive activity.Other examples of diluents are sodium chloride and sodium carbonate.Diluents such as the silicates exemplified by sodium metasilicate andsodium silicates wherein the ratio of Na O to SiO is from about 1.621 toabout 3.2:1; borax; clays such as kaolin, the montmorillonites, andbentonites; silica sol; titanium oxide; colloidal aluminum hydroxide;and ammonium carbonate can also be used; however, it is preferred thatthe major proportion of the diluent be an alkali metal sulfate, whichcan be considered an inert material.

The third component of the second group is an alkali metal (generally,Na or K) carboxymethylcellulose, in particular those having about 0.5 toabout 0.8 carboxymethyl group per cellulose unit. This component isconsidered an organic builder and as noted in U.S. Pat. No. 3,360,470referred to above provides the antiyellowing efiect for the quaternaryammonium softener.

The proportions of the second group of components which are by weightbased on the total weight of components introduced into the crutcher areas follows: alkali metal phosphate builder salt-about 13 percent toabout 45 percent and preferably 27 percent to 33 percent; dilventabout 7percent to about 25 percent and preferably 17 percent to about 23percent; and an alkali metal carboxymethylcellulose about 0.3 percent toabout 4.5 percent and preferably about 0.7 percent to about 2.5 percent.

In addition to the stated proportions, the proportions should beselected in a corresponding ratio so that there will be a sufficientamount of each component to provide more than 47 percent solids in thecrutcher composition. it should be noted that even through 59-60to 65percent solids are generally considered the most desirable forspray-drying, all of the solids percentages above 47 percent andpreferably about 50 percent are important because the bulk density ofthe composition after spray-drying is dependent upon the percentage ofsolids resulting from the crutching operation. Although it is notgenerally the case, there are some instances when it is commerciallynecessary to achieve a bulk density which will result from a lowersolids percentage. However, this does not in any case normally go belowthe 50 percent solids level. About 65 percent solids is the upperpractical limit for spraydrying because the high solids content becomestoo difficult to pump; however, higher levels of solids can be crutchedwithin the process of this invention, if desired.

Crutching time is generally from about 5 minutes to an hour or more withabout 20 to 40 minutes being most desirable. Time is not critical and ithas been found that about 30 minutes provides satisfactory homogeneity.Times greater than an hour provide no advantage and shorter than 5minutes contribute to waste because of settling.

The spray-drying equipment used is just as conventional as the crutchingequipment. It includes spray nozzles, a high pressure pump, an air spraysystem, a heater for the air, and a dust separator. Two types of systemsmake use of this equipment. They are known as parallelcurrent andcountercurrent drying and of these two systems the countercurrent systemis the most desirable; however, in many cases, both systems are used totake advantage of each.

Conventional colorants, perfumes, brighteners, and bluing agents can beadded if desired. The amounts of these substances introduced into thesoftener-detergent composition are obviously such that they will notadversely affect the desired properties. The amounts of all of thesesubstances taken together add up to less than 2 percent by weight of thetotal weight of the crutcher composition and preferably less than 1percent. The colorants are usually in the form of dyes. Examples of thebrighteners are stilbene, triazole, and benzidine sulfone compositions,the stilbene and triazole compositions in combination being preferred.These components are, of course, not an essential part of thesoftener-detergent composition used in the process of this invention.The colorant and perfume are preferably added during or afterspray-drying whereas the brighteners are added to the crutcher mixture.The bluing agent is usually added to the crutcher mixture after thewater and it is a preferred component because of its antiyellowingcontribution. An example of a bluing agent is ultramarine blue which hasbeen found to be stable to light, alkali, and bleach and is insoluble inwater. Ultramarine blue is a well-known blue pigment occurring naturallyas the mineral lapis lazuli and can be synthesized by igniting a mixtureof kaolin, sodium carbonate or sulfate, sulfur, and carbon. Themicropulverized, synthetic ultramarine blues have proved satisfactory.

The proportions of components which can be present in the final productin percent by weight based on the total weight of the final compositionare as follows: waterabout 5 percent to about 15 percent and preferablyabout 6.5 percent to about 12.5 percent; nonionic detergentabout 5percent to about 30 percent and preferably about 7 percent to about l2percent; quaternary ammonium salt-about 2 percent to about 8 percent andpreferably about 4 percent to about 6 percent; alkali metal phosphatebuilder salts about 20 percent to about 65 percent and preferably about40 percent to about 48percent; dilventabout 10 percent to about 37.5percent and preferably about 25 percent to about 35percent; an alkalimetal carboxymethylcelluloseabout 0.5 percent to about 5.33 percent andpreferably about 1 percent to about 3.5 percent; colorant, perfumes,brighteners, and bluing agentstotal weight 0 percent to about 2 percentand preferably 0 percent to about 1 percent; bleaching agent-0 percentto about 10 percent and preferably 0 percent to about 5 percent.

The following examples are illustrative of the invention. Parts andpercentages are by weight.

EXAMPLE I The following crutcher formula (59.5 percent solids) was usedin this example and the components were introduced in consecutive orderas numbered:

Percent in Final Component Percent in Crutcher S ray-dried Product I.water (exclusive of 37.640

water mentioned below) 2. ultramarine blue 3. nonionic detergent (nnnylphenol--ethylene oxide condensate having an average of 9 ethylene oxidegroups er molecule) softener (dimethyl dihydrogenated ditallowquaternary ammonium chloride) anhydrous sodium sulfate .a 43.5 percentsolution of sodium silicate in water; ratio of Na, to SiO, is 2.35:]

(silicate) sodium tripolyphosphate 29.735

. a 75 ercent dispersion of sodium carboxymethylcellulose (CMC) in water(CMC) 9. a stilbene brightener 10. a triazole brightener agitation (350rpm), after which the CMC and the brighteners were added. The crutchingtime was 30 minutes.

The slurry was then pumped with a triplex pump into a spray tower whereit was met with a countercurrent of hot air. The dried particles droppedto a conveyor and were transported to an air lift, which passed thegranules along to a separator. Screening, perfuming, and packagingfollowed.

The spray tower conditions were as follows:

tower inlet air temperature SUP-520 F. tower outlet air temperaturel85-269 1-. nozzle size 10 number of noulcs 4 triplex pressure 660p.s.i.g. Productcup weight 81-100 grams The spray-dried product wasfound to perform well in softening and laundering.

EXAMPLE 11 The same crutcher steps and conditions as in example 1 arefollowed except the order of addition was water, blue, sulfate,silicate, tripolyphosphate, nonionic detergent, CMC and brighteners, andquaternary ammonium salt. Agitation is used for all ingredients exceptthe nonionic detergent. The 180 F. temperature was invoked before theaddition of sulfate.

This procedure produces gelation EXAMPLE 111 The same crutcher steps andconditions prevalent in example l are followed except that instead of180 F., a temperature of 175 F. is used.

This procedure produces a gelation EXAMPLE [V The same crutcher stepsand conditions are followed as in examples 11 and 111 except that ineach case proportions are adjusted to reduce the level of crutchersolids to 47 percent.

No gelation occurs.

EXAMPLE V The same crutcher steps and conditions are followed as inexample 1 except that proportions are adjusted to reduce the level ofcrutcher solids to 50 percent.

No gelation occurs.

EXAMPLE Vl Example 1 is repeated except that the proportions areadjusted to obtain 65 percent solids.

No gelation occurs.

EXAMPLE Vll Example 1 is repeated except that the CMC and brightenersare added just before the tripolyphosphate.

No gelation occurs.

EXAMPLE V111 The procedure of examples [1 and 111 is followed todetermine which of the components has an effect on gelation. This isaccomplished by elimination of components. It is ascertained that theelimination of either the nonionic detergent, the quaternary ammoniumsalt or the phosphate from the crutching formula results in no gelation.

We claim:

1. A process for preparing a spraydricd granular softenerdetergcntcomposition consisting essentially of (a) about 2 percent to about 8percent by weight ofa quaternary ammonium textile softener representedby the general formula It: t

l lh N-Ri X- wherein R and R are alkyl groups each containing from 1 to3 carbon atoms; R and R are alkyl groups each containing from 12 to 22carbon atoms; and X is selected from the group consisting of chlorine,bromine, and methyl sulfate; (12) about 5 percent to 30 percent byweight of a water-soluble nonionic detergent having a hydrophobic groupof 8 to 30 carbon atoms condensed with 5 to 30 moles of ethylene oxide;(c) about 20 percent to 65 percent of a sodium or potassium inorganicphosphate builder salt; and (d) 5 to 15 percent water which comprisesthe steps of: l admixing water, said nonionic detergent, and quaternaryammonium softener to form an aqueous mixture wherein the quaternarysoftener is homogeneously dispersed; (2) introducing a sodium orpotassium inor ganic phosphate builder salt into said aqueous mixturewhereby a mixture containing more than 50 percent of solids is formed,the temperature of the mixture being at least about 180 F. and below 212F. at the time said phosphate is introduced therein; and (3) spraydrying the mixture of step 2.

2. A process in accordance with claim 1 wherein said water, saidnonionic, and said softener are admixed at a temperature in the range ofabout F. to about F. and the temperature of said mixture is raised to atleast about F. prior to the introduction of said phosphate.

3. A process in accordance with claim 1 wherein said water, saidnonionic, and said softener are admixed at a temperature ofat least 180F.

4. A process in accordance with claim 1 wherein at least onewater-soluble inorganic diluent selected from the group consisting ofsodium sulfate, potassium sulfate, sodium carbonate, sodium chloride andsodium silicate is introduced prior to, simultaneously with, or aftersaid introduction of said phosphate, the amount of said diluent beingsufficient to provide 10 to 37.5 percent by weight of said diluent inthe spraydried product.

5. A process in accordance with claim 1 wherein a sodium or potassiumcarboxymethylcellulose salt is introduced prior to, simultaneously withor after said introduction of said phosphate, the amount of saidcellulose being sufficient to provide 0.5 to about 5.33 percent byweight of said cellulose in the spray-dried product.

6. A process in accordance with claim 1 wherein the temperature of themixture of step 1 is about 180 F. to about F. at the time said phosphateis introduced.

7. A process in accordance with claim 1 wherein said phosphate buildersalt is sodium or potassium tripolyphosphate.

8. A process in accordance with claim 4 wherein said diluent is sodiumor potassium sulfate.

9. A process in accordance with claim 8 wherein said sulfate is addedafter said phosphate salt and a sodium or potassiumcarboxymethylcellulose is introduced thereafter, the amount of saidcellulose being sufficient to provide 05 percent to about 5.33 percentby weight thereof in the spray-dried product. l

10. A process in accordance with claim 9 wherein the mixture formed andspray dried contains about 59 percent to about 65 percent solids byweight.

2. A process in accordance with claim 1 wherein said water, saidnonionic, and said softener are admixed at a temperature in the range ofabout 130* F. to about 160* F. and the temperature of said mixture israised to at least about 180* F. prior to the introduction of saidphosphate.
 3. A process in accordance with claim 1 wherein said water,said nonionic, and said softener are admixed at a temperature of atleast 180* F.
 4. A process in accordance with claim 1 wherein at leastone water-soluble inorganic diluent selected from the group consistingof sodium sulfate, potassium sulfate, sodium carbonate, sodium chlorideand sodium silicate is introduced prior to, simUltaneously with, orafter said introduction of said phosphate, the amount of said diluentbeing sufficient to provide 10 to 37.5 percent by weight of said diluentin the spray-dried product.
 5. A process in accordance with claim 1wherein a sodium or potassium carboxymethylcellulose salt is introducedprior to, simultaneously with or after said introduction of saidphosphate, the amount of said cellulose being sufficient to provide 0.5percent to about 5.33 percent by weight of said cellulose in thespray-dried product.
 6. A process in accordance with claim 1 wherein thetemperature of the mixture of step 1 is about 180* F. to about 190* F.at the time said phosphate is introduced.
 7. A process in accordancewith claim 1 wherein said phosphate builder salt is sodium or potassiumtripolyphosphate.
 8. A process in accordance with claim 4 wherein saiddiluent is sodium or potassium sulfate.
 9. A process in accordance withclaim 8 wherein said sulfate is added after said phosphate salt and asodium or potassium carboxymethylcellulose is introduced thereafter, theamount of said cellulose being sufficient to provide 0.5 percent toabout 5.33 percent by weight thereof in the spray-dried product.
 10. Aprocess in accordance with claim 9 wherein the mixture formed and spraydried contains about 59 percent to about 65 percent solids by weight.